CN101538296A - Active ingredients of camptosorus sibiricus, and extraction method and use of same - Google Patents
Active ingredients of camptosorus sibiricus, and extraction method and use of same Download PDFInfo
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Abstract
The invention belongs to the technical field of medicaments and provides active ingredients of Chinese herbal medicine camptosorus sibiricus and an extraction method and use of the same. The extraction method comprises a water extraction method, an alcohol extraction method, a macroporous resin purification method and a solvent extraction method. The main active ingredients of an extract obtained by the method are total flavonoids, total momordica saponins and total organic acids, wherein the content of the total flavonoids is 1 to 35 percent, the content of the total momordica saponins is 1 to 25 percent and the content of the total organic acids is 1 to 3 percent. The invention also provides a method for preparing the camptosorus sibiricus into a proper formulation directly or by mixing with solid or liquid commonly used for preparations of the type in pharmaceutics. The active ingredients of the camptosorus sibiricus and the preparation thereof have functions of treating thromboangiitis obliterans, nephritis, traumatism and bleeding, metrorrhagia, neurodermitis, hemiplegia caused by cerebral embolism and diabetes-related complications. The extraction method is simple, easy to implement and low in cost. And the extract obtained is free from toxic and side effects.
Description
Technical field:
The invention belongs to medical technical field, relate to extraction process of effective component and the purposes of herbal medicine walking fern, and the production and processing method of active ingredients of camptosorus sibiricus preparation.
Background technology:
Walking fern (Camptosorus sibiricus Rupr.) has another name called Herba Camptosori Sibirici, Radix Rhodiolae Yunnanensis, and the grass of passing a bridge is Aspleniaceae, walking fern belongs to per nnial herb.Totally two kinds in this genus whole world, in homemade a kind of.Walking fern is a kind of traditional herbal medicines, among the peoplely is used for the treatment of traumatic hemorrhage, uterine hemorrhage, and thromboangiitis obliterans, ephritis, hemiplegia that neurodermatitis, cerebral embolism cause and diabetic complication etc. have definite curative effect.Experiment shows that this herbal medicine toxicity is very little, and blood pressure is not had obvious influence, and long term administration is not seen detrimentally affect to the rabbit liver function.The extraction of its effective constituent and utilize its effective constituent process for processing to become preparation that report is not arranged.
Summary of the invention:
The object of the present invention is to provide the extracting method of active ingredients of camptosorus sibiricus, and utilize its several preparations of effective constituent process for processing, with its as the treatment thromboangiitis obliterans, ephritis, traumatic hemorrhage, uterine hemorrhage, the hemiplegia that neurodermatitis, cerebral embolism cause and the medicine of diabetic complication.
Active ingredients of camptosorus sibiricus is composed as follows:
The present invention is achieved by the following scheme: the preparation method of described active ingredients of camptosorus sibiricus divides four kinds:
Method 1: after getting the crude drug impurity elimination, adding 15 to 30 times of water gagings decoctions is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 6-24 hour to precipitation, remove precipitation, get supernatant liquor and add ethanol sedimentation 1-2 time, alcohol concn is at 50%-90% in the control extracting solution, complete at 0-10 ℃ of following stand at low temperature 12-48 hour to precipitation, filter once more, filtrate recycling ethanol is not to there being the alcohol flavor, and the gained supernatant liquor carries out separation and purification through macroporous resin (HPD 100 or D101), respectively with water, 5%-30% ethanol, 30%-60% ethanol, 60%-95% ethanol elution, 5%-30% ethanol elution thing is an effective constituent group 1,30%-60% ethanol elution thing is an effective constituent group 2, and 60%-95% ethanol elution thing is an effective constituent group 3, and the three is combined as the walking fern effective extract by amounting to the raw medicinal herbs amount at 1: 1: 1.
Method 2: after getting the crude drug impurity elimination, the ethanol that adds the 5%-95% of 15 to 30 times of amounts decocts and is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 12-24 hour to precipitation, remove precipitation, the gained supernatant liquor carries out separation and purification through macroporous resin (HPD 100 or D101), respectively with water, 5%-30% ethanol, 30%-60% ethanol, the 60%-95% ethanol elution, 5%-30% ethanol elution thing is an effective constituent group 1,30%-60% ethanol elution thing is an effective constituent group 2,60%-95% ethanol elution thing is an effective constituent group 3, and the three is combined as the walking fern effective extract by amounting to the raw medicinal herbs amount at 1: 1: 1.
Method 3: after getting the crude drug impurity elimination, the ethanol that adds the 5%-95% of 15 to 30 times of amounts decocts and is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 12-24 hour to precipitation, remove precipitation, get supernatant liquor use respectively twice of sherwood oil (or hexanaphthene, normal hexane), ethyl acetate, n-butanol extraction above to extraction fully.Reclaim solvent, gained n-butanol extraction layer is through macroporous resin (HPD 100 or D101) purifying, respectively with water, 5%-95% ethanol, ethanol elution, 5%-95% ethanol elution thing is an effective constituent component 1, and the ethyl acetate extraction layer is an effective constituent group 2, and the two is combined as the walking fern effective extract by amounting to the raw medicinal herbs amount at 1: 1.
Method 4: after getting the crude drug impurity elimination, adding 15 to 30 times of water gagings decoctions is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 6-24 hour to precipitation, remove precipitation, get supernatant liquor use respectively twice of sherwood oil (or hexanaphthene, normal hexane), ethyl acetate, n-butanol extraction above to extraction fully.Reclaim solvent, gained n-butanol extraction layer is through macroporous resin purification, respectively with water, 5%-95% ethanol, ethanol elution, 5%-95% ethanol elution thing is an effective constituent component 1, the ethyl acetate extraction layer is an effective constituent group 2, and the two is combined as the walking fern effective extract by amounting to the raw medicinal herbs amount at 1: 1.
In the gained active ingredients of camptosorus sibiricus extract, general flavone content is 1%-35%, and total saponin content is 1%-25%, and total phenolic content is 1%-3%.
By aforesaid method as seen, the active ingredients of camptosorus sibiricus extract is made up of total flavones, total saponins and total phenolic acid, can prepare by above-mentioned four kinds of methods, can sketch to be method one: water is carried-depositing in water-alcohol precipitation-macroporous resin segmentation purifying; Method two: alcohol extracting-depositing in water-macroporous resin segmentation purifying; Method three: alcohol extracting-solvent stage extraction-macroporous resin purification; Method four: water is carried-solvent stage extraction-macroporous resin purification.
That extract of the present invention has is anti-oxidant, remove free radical, aldose reductase suppresses, the vasodilation isoreactivity, can be used for treating the treatment of diseases such as thromboangiitis obliterans, diabetic ephritis, traumatic hemorrhage.Utilize partial monosomy compound in the active ingredients of camptosorus sibiricus extract that the present invention obtains have anti-oxidant significantly, remove the activity that free radical, aldose reductase suppress.
Advantage of the present invention is as follows:
(1) this preparation method gained walking fern extract component is clear and definite, compound 1-12 wherein, and 19-21 is the walking fern endemic element, quality controllability is strong.
(2) gained active ingredients of camptosorus sibiricus extract of the present invention is made up of three kinds of dissimilar natural products, has many target spot synergies and the low advantage of toxic side effect.
(3) easy, the easy row of preparation method extracts fully, is suitable for industrial production
(4) the active ingredients of camptosorus sibiricus extract is significantly active, and determined curative effect can effectively reduce the Chinese medicine dose.
Description of drawings:
Fig. 1 is partial monosomy compound quasi-SOD active testing result
*：IC50＜10uM
Fig. 2 is a partial monosomy compound free radical scavenging activity test result
*：IC50＜15uM
Fig. 3 is a partial monosomy compound aldose reductase inhibition activity test result
*：IC50＜50uM
Embodiment:
According to effective constituent preparation method 1
(1) gets dry walking fern herb 10kg, remove impurity, dust
(2) water of adding medicinal material and 18 times of amounts in the traditional Chinese medicine extraction jar, heated and boiled extracts twice, each 2 hours.
(3) merge extracted twice liquid, be concentrated into 20L, extremely precipitation was complete in 24 hours 4 ℃ of following stand at low temperature, removed precipitation.
(4) get supernatant liquor and add ethanol, regulate determining alcohol to 50%, extremely precipitation was complete in 24 hours 10 ℃ of following stand at low temperature, filtered once more, and filtrate recycling ethanol to nothing alcohol is distinguished the flavor of.
(5) sample is distinguished water (8V to the non-polar macroporous resin post on the supernatant liquor
R), 20% ethanol (4V
R), 60% ethanol (4V
R), 90% ethanol (4V
R) gradient elution, must wash thing and discard, 20% ethanol elution thing, 60% ethanol elution thing, 90% ethanol elution thing are according to amounting to the crude drug amount 1: 1: 1 mixed, get the walking fern effective extract, wherein general flavone content is 30%, and total saponin content is 20%, and total phenolic content is 1%.
According to effective constituent preparation method 2
(1) gets dry walking fern herb 5kg, remove impurity, dust
(2) 70% ethanol of adding medicinal material and 20 times of amounts in the traditional Chinese medicine extraction jar, heating and refluxing extraction three times was respectively 2 hours, and 1.5 hours, 1 hour.
(3) merge No. three extracting solutions, be concentrated into 8L, extremely precipitation was complete in 12 hours 4 ℃ of following stand at low temperature, removed precipitation.
(5) sample is distinguished water (8V to the non-polar macroporous resin post on the supernatant liquor
R), 30% ethanol (4V
R), 70% ethanol (4V
R), 95% ethanol (4V
R) gradient elution, must wash thing and discard 30% ethanol elution thing, 70% ethanol elution thing, 95% ethanol elution thing according to amounting to the crude drug amount 1: 1: 1 mixed, get the walking fern effective extract, wherein general flavone content is 33%, total saponin content is 20%, and total phenolic content is 2%.
According to effective constituent preparation method 3
(1) gets dry walking fern herb 6kg, remove impurity, dust
(2) 75% ethanol of adding medicinal material and 25 times of amounts in the traditional Chinese medicine extraction jar, heating and refluxing extraction three times was respectively 2 hours, and 1.5 hours, 1 hour.
(3) merge No. three extracting solutions, be concentrated into 10L, extremely precipitation was complete in 20 hours 4 ℃ of following stand at low temperature, removed precipitation.
(4) supernatant liquor is with equal-volume sherwood oil, ethyl acetate, n-butanol extraction four times.Get petroleum ether extract 320 grams, acetic acid ethyl ester extract 60 grams, n-butyl alcohol extract 180 grams.Reclaim lyase, the gained n-butyl alcohol extract is further through macroporous resin purification, and respectively with water, 95% ethanol elution, reclaim under reduced pressure lyase get 95% ethanol elution thing, 140 grams.95% ethanol elution thing and acetic acid ethyl ester extract by amounting to crude drug than 1: 1 mixed, are obtained the active ingredients of camptosorus sibiricus extract.Get the walking fern effective extract, wherein general flavone content is 28%, and total saponin content is 21%, and total phenolic content is 1.5%.
According to effective constituent preparation method 4
(1) gets dry walking fern herb 10kg, remove impurity, dust
(2) water of adding medicinal material and 30 times of amounts in the traditional Chinese medicine extraction jar, heated and boiled is extracted three times, was respectively 2 hours, 1.5 hours, 1 hour.
(3) merge No. three extracting solutions, be concentrated into 15L, extremely precipitation was complete in 12 hours 4 ℃ of following stand at low temperature, removed precipitation.
(4) supernatant liquor is with equal-volume hexanaphthene, ethyl acetate, n-butanol extraction four times.Get petroleum ether extract 510 grams, acetic acid ethyl ester extract 70 grams, n-butyl alcohol extract 310 grams.Reclaim lyase, the gained n-butyl alcohol extract is further through macroporous resin purification, and respectively with water, 90% ethanol elution, reclaim under reduced pressure lyase get 95% ethanol elution thing, 240 grams.95% ethanol elution thing and acetic acid ethyl ester extract by amounting to crude drug than 1: 1 mixed, are obtained the active ingredients of camptosorus sibiricus extract.Get the walking fern effective extract, wherein general flavone content is 26%, and total saponin content is 24%, and total phenolic content is 1.1%.
Adopt the SOD test kit that the monomeric compound in the extract has been carried out the anti-oxidant activity test
Experimental technique is as follows
Experimental result: see Table 1
Adopt DPPH free radical scavenging screening model, the monomeric compound in the extract has been carried out the free radical scavenging activity test
Experimental technique is as follows
Experimental result: see Table 1
Adopt aldose reductase inhibitor (ARI) screening model, the monomeric compound in the extract has been carried out the aldose reductase inhibition activity test.
Experimental technique is as follows
A 180mM Na-K phosphate buffered saline buffer 225 μ L
B?1.0M?Li
2SO4 50μL
C 10mM DL-glyceraldehyde (sample sets parallel 2) 50 μ L
H
2O (blank group) 50 μ L
E sample (sample sets and blank group are respectively) 25 μ L
The A-E mixed solution is at 30 ℃ of following heating in water bath 3min, add 0.3M NADPH 50 μ L, under 30 ℃ of water-baths, heat 30min again, add 0.5N HCl 150 μ L, add 10mMimidazole 500 μ L (containing 6N NaOH) again, heat 20min under 60 ℃ of water-baths, room temperature is placed, add 200 μ L reaction solutions in 96 orifice plates respectively, fluorescence detector detects (λ
Ex360nm, λ
Em460nm)
Experimental result: see Table 1
Get walking fern effective extract (preparation method such as embodiment 1) dry, pulverize, cross 80 mesh sieves, directly or add suitable diluents (dextrin, microcrystalline cellulose etc.) can capsule.
Get walking fern effective extract (preparation method such as embodiment 2) and add thinner (dextrin, starch etc.), dry, pulverizing, granulation, compressing tablet or pill agent in 1: 1～1: 4 ratio.
Claims (6)
1, active ingredients of camptosorus sibiricus is characterized in that: comprise trifolitin type flavonoid glycoside, cyclic-ahltin type triterpenoid saponin, small molecules phenolic acids; The structural formula of this effective constituent is:
2, a kind of extracting method of active ingredients of camptosorus sibiricus as claimed in claim 1 is characterized in that: its extracting method is as follows:
After getting the crude drug impurity elimination, adding 15 to 30 times of water gagings decoctions is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 6-24 hour to precipitation, remove precipitation, get supernatant liquor and add ethanol sedimentation 1-2 time, alcohol concn is at 50%-90% in the control extracting solution, complete at 0-10 ℃ of following stand at low temperature 12-48 hour to precipitation, filter once more, filtrate recycling ethanol is not to there being the alcohol flavor, and the gained supernatant liquor carries out separation and purification through macroporous resin, respectively with water, 5%-95% ethanol, ethanol elution, 5%-95% ethanol elution thing is the effective constituent group;
Or after getting the crude drug impurity elimination, the ethanol that adds the 5%-95% of 15 to 30 times of amounts decocts and is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 12-24 hour to precipitation, remove precipitation, get supernatant liquor and add ethanol sedimentation 1-2 time, alcohol concn is at 50%-90% in the control extracting solution, complete at 0-10 ℃ of following stand at low temperature 12-48 hour to precipitation, filter once more, filtrate recycling ethanol is not to there being the alcohol flavor, and the gained supernatant liquor carries out separation and purification through macroporous resin, respectively with water, 5%-95% ethanol, ethanol elution, 5%-95% ethanol elution thing is the effective constituent group;
Or after getting the crude drug impurity elimination, the ethanol that adds 5%-95% decocts and is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 12-24 hour to precipitation, remove precipitation, get supernatant liquor use respectively twice of sherwood oil (or hexanaphthene, normal hexane), ethyl acetate, n-butanol extraction above to extraction fully.Reclaim solvent, gained ethyl acetate extraction layer and n-butanol extraction layer are the effective constituent group;
Or after getting the crude drug impurity elimination, adding 15 to 30 times of water gagings decoctions is no less than twice, each extraction time is no less than 1 hour, extracting solution is concentrated into 1/5th to 1/20th of medicine liquid volume, complete at 0-10 ℃ of following stand at low temperature 6-24 hour to precipitation, remove precipitation, get supernatant liquor use respectively twice of sherwood oil (or hexanaphthene, normal hexane), ethyl acetate, n-butanol extraction above to extraction fully.Reclaim solvent, gained ethyl acetate extraction layer and n-butanol extraction layer are the effective constituent group.
3, the extracting method of active ingredients of camptosorus sibiricus according to claim 2 is characterized in that: in the described effective constituent group: general flavone content is 1%-35%, and total saponin content is 1%-25%, and total phenolic content is 1%-3%.
4, the extracting method of active ingredients of camptosorus sibiricus according to claim 2 is characterized in that: can also be with the spray-dried pulverulent solids of making of active ingredients of camptosorus sibiricus group extracting solution.
5, the extracting method of active ingredients of camptosorus sibiricus according to claim 4 is characterized in that: its spraying drying condition is: the preheating of air to 280 that sprays into ± 20 ℃, the air pressure that sprays into is 3-6kg/cm
2, dry room temp remains on 120 ± 20 ℃, extracts total active constituent content＞50% in the powder.
6, active ingredients of camptosorus sibiricus is in preparation treatment thromboangiitis obliterans, ephritis, traumatic hemorrhage, uterine hemorrhage, the application in hemiplegia that neurodermatitis, cerebral embolism cause and the diabetes complicated disease drug.
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| CN104961791A (en) * | 2015-06-05 | 2015-10-07 | 中国科学院西北高原生物研究所 | Novel triterpene compound in potentilla anserina, and preparation method and application thereof |
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| CN109796511A (en) * | 2019-03-05 | 2019-05-24 | 山东省药学科学院 | A kind of new iridoid and preparation method thereof and medical usage |
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| CN102526130A (en) * | 2011-11-07 | 2012-07-04 | 卢建立 | Application of walking fern and liver function revised tea |
| CN103059069A (en) * | 2012-12-13 | 2013-04-24 | 大兴安岭林格贝有机食品有限责任公司 | Novel technique method for extracting general flavone from wild walking fern |
| CN103059069B (en) * | 2012-12-13 | 2016-05-25 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of process of extracting general flavone from wild walking fern |
| CN104961791A (en) * | 2015-06-05 | 2015-10-07 | 中国科学院西北高原生物研究所 | Novel triterpene compound in potentilla anserina, and preparation method and application thereof |
| CN104961791B (en) * | 2015-06-05 | 2017-03-08 | 中国科学院西北高原生物研究所 | A kind of new triterpenoid, preparation method and purposes in Radix potentillae anserinae |
| CN105613595A (en) * | 2015-12-22 | 2016-06-01 | 新乡医学院第一附属医院 | Cleaning disinfectant for CT equipment and preparation method and application thereof |
| CN105613595B (en) * | 2015-12-22 | 2018-03-09 | 新乡医学院第一附属医院 | A kind of cleaning disinfection liquid for CT equipment and its preparation method and application |
| US11608353B2 (en) * | 2016-07-27 | 2023-03-21 | The University Of British Columbia | Amylase inhibitor compounds, methods of their use and compositions thereof |
| CN109796511A (en) * | 2019-03-05 | 2019-05-24 | 山东省药学科学院 | A kind of new iridoid and preparation method thereof and medical usage |
| CN109796511B (en) * | 2019-03-05 | 2021-10-22 | 山东省药学科学院 | Novel iridoid compound and preparation method and medical application thereof |
| CN111808160A (en) * | 2020-07-10 | 2020-10-23 | 山东省药学科学院 | New cycloartane type saponin-9, 19-seco-9, 11-ene derivative and its preparing method and use |
| CN111808160B (en) * | 2020-07-10 | 2022-08-09 | 山东省药学科学院 | New cycloartane type saponin-9, 19-seco-9, 11-ene derivative and its preparing method and use |
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